Synthesis method of hydroxyalkyl tertiary ammonium beta-hydroxyalkyldienediaminocaproate

A technology of diaminocaproic acid hydroxyalkyl tertiary amine and diaminocaproic acid, which is applied in the field of antirust additive synthesis, can solve the problems of few product varieties and limited application coverage, achieve strong antirust effect and improve anodic polarization performance, corrosion inhibitory effect

Active Publication Date: 2014-10-22
山东蓝盟防腐科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, compared with advanced countries, China's gas-phase anti-rust technology still has the problems of fewer product varieties and limited application ...

Method used

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  • Synthesis method of hydroxyalkyl tertiary ammonium beta-hydroxyalkyldienediaminocaproate
  • Synthesis method of hydroxyalkyl tertiary ammonium beta-hydroxyalkyldienediaminocaproate
  • Synthesis method of hydroxyalkyl tertiary ammonium beta-hydroxyalkyldienediaminocaproate

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Experimental program
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Effect test

Embodiment 1

[0022] In a four-necked flask equipped with a stirring device, a reflux condensing device and a thermometer, add 159 grams of benzene, add 2 grams of zinc chloride, 1 gram of zinc oxide and 106 grams of caprolactam, and slowly add 29 grams of chlorinated epoxy Propane, add a saturated aqueous solution of sodium carbonate to the reaction mixture, raise the temperature to 80°C-90°C and continue the reflux reaction for 7 hours. During the reaction, use an acid-binding agent to control the pH at 8.5-9.5 to generate biscaprolactam-2-ol, and the reaction is complete Afterwards, cool to 30°C, stop stirring, add 120 grams of 47% sodium hydroxide solution to the reaction mixture to dilute and hydrolyze the reaction, the reaction mixture is divided into two layers, the upper layer is an organic phase, and the lower layer is separated to obtain a liquid β-hydroxyalkane Diethylene diaminocaproic acid sodium solution, slowly add 30% sulfuric acid solution to the β-hydroxyalkylene diaminocap...

Embodiment 2

[0024] In a four-neck flask equipped with a stirring device, a reflux condensing device and a thermometer, add 165 grams of benzene, 2 grams of zinc chloride, 2 grams of zinc oxide and 82.5 grams of caprolactam, and slowly add 31 grams of chlorinated epoxy Butane, add saturated aqueous solution of sodium carbonate to the reaction mixture, raise the temperature to 85°C-95°C and continue the reflux reaction for 6 hours. During the reaction, use an acid-binding agent to control the pH at 8.5-9.5 to generate biscaprolactam-2-ol. After completion, cool to 40°C, stop stirring, add 100 grams of 44% sodium hydroxide solution to the reaction mixture for dilution and hydrolysis reaction, the reaction mixture is divided into two layers, the upper layer is the organic phase, and the lower layer is separated to obtain liquid β-hydroxyl Sodium alkylene diaminocaproate solution, slowly add 20% hydrochloric acid to the sodium β-hydroxyalkylene diaminocaproate solution, adjust the pH to about 1...

Embodiment 3

[0026] In a four-neck flask equipped with a stirring device, a reflux condensing device and a thermometer, add 176 grams of benzene, 1.5 grams of zinc chloride, 1.2 grams of zinc oxide and 70.5 grams of caprolactam, and slowly add 33 grams of chlorinated epoxy Butane, add saturated aqueous solution of sodium carbonate to the reaction mixture, raise the temperature to 90°C-95°C and continue the reflux reaction for 8 hours. During the reaction, use an acid-binding agent to control the pH at 8.5-9.5 to generate biscaprolactam-2-ol. After completion, cool to 20°C, stop stirring, add 95 grams of 40% sodium hydroxide solution to the reaction mixture for dilution and hydrolysis reaction, the reaction mixture is divided into two layers, the upper layer is an organic phase, and the lower layer is separated to obtain liquid β-hydroxyl Sodium alkylene diaminocaproate solution, slowly add 35% sulfuric acid solution to the sodium β-hydroxyalkylene diaminocaproate solution, adjust the pH to ...

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Abstract

The invention discloses a synthesis method of hydroxyalkyl tertiary ammonium beta-hydroxyalkyldienediaminocaproate. The synthesis method comprises that chloroepoxyalkane and a caprolactam group undergoes a heating backflow reaction with stirring in the presence of benzene as a solvent and zinc chloride and zinc hydroxide as catalysts to produce dicaprolactam-2-ol, a sodium hydroxide solution is added into the reaction mixture, a lower layer is separated so that a sodium beta-hydroxyalkyldienediaminocaproate solution is obtained, an acid solution is slowly added into the sodium beta-hydroxyalkyldienediaminocaproate solution, a PH value of the mixed solution is adjusted to about 1.0, and the separated beta-hydroxyalkyldienediaminocaproic acid is added into the hydroxyalkyl tertiary amine so that the hydroxyalkyl tertiary ammonium beta-hydroxyalkyldienediaminocaproate is obtained. The hydroxyalkyl tertiary ammonium beta-hydroxyalkyldienediaminocaproate has multiple active adsorption centers, can improve anodic polarization performances and has corrosion inhibition effects. The hydroxyalkyl tertiary ammonium beta-hydroxyalkyldienediaminocaproate has combined characteristics of two amido groups, two carboxyl groups and metals, and has strong antirust effects and antiwear and antifriction effects.

Description

technical field [0001] The invention relates to the technical field of antirust additive synthesis, in particular to a synthesis method of β-hydroxyalkylene diaminocaproic acid hydroxyalkyl tertiary amine. Background technique [0002] Metal antirust is a complex system engineering. The antirust effect not only depends on the quality of the antirust product itself, but also involves the cleanness and dryness of the metal surface, the quality of the surface material, the environment of the work site, the quality of the operator's operation, whether the process is scientific, There are many aspects such as whether there is any damage during storage and transportation. The anti-rust material is only one of the factors. The occurrence of rust does not necessarily mean that the quality of the anti-rust product is defective, but if the anti-rust product is not used or cannot be used scientifically and correctly, rust will definitely occur. Vapor-phase anti-rust is a science that ...

Claims

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Application Information

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IPC IPC(8): C07C227/18C07C229/12C07C213/08C07C215/12C23F11/02
Inventor 修建东刘方旭
Owner 山东蓝盟防腐科技股份有限公司
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